1,4-Dioxane hydrochloride → HCID 21137721, 화합물

HRID 1358581노트

반응식

HRID 1358581 반응식
[CH3:1][O:2][C:3](=[O:30])[C@H:4]([CH3:29])[NH:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:13][C:14]([O:16]C(C)(C)C)=[O:15])=[CH:8][C:7]=1[C:21](=[O:28])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.Cl.O1CCOCC1>O1CCOCC1>[CH3:1][O:2][C:3](=[O:30])[C@H:4]([CH3:29])[NH:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:13][C:14]([OH:16])=[O:15])=[CH:8][C:7]=1[C:21](=[O:28])[C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1

참가 물질

4

반응물 2

HCID 204431481,4-Dioxane hydrochlorideHCID 21137722HCID 21137722, 화합물

생성물 1

HCID 21137721HCID 21137721, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A mixture of 4-t-butoxycarbonylmethoxy-N-(2-benzoylphenyl)alanine methyl ester (1.4 g), 4N hydrogen chloride/dioxane (10 ml) and dioxane (10 ml) was stirred at room temperature for 3 hours and allowed to stand overnight. The reaction mixture was concentrated under reduced pressure. To the residue was added toluene and the mixture was concentrated under reduced pressure. The residue was chromatographed on a silica gel column (LiChroprepDIOL (Merck)) using hexane: ethyl acetate=2:1−1:1 as the eluant to afford the title compound (0.87 g, Rf=0.53: thin layer chromatography on a silica gel plate using hexane: ethyl acetate=3:2 as the eluant).

후처리

  1. waitto stand overnight
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. additionTo the residue was added toluene
  4. concentrationthe mixture was concentrated under reduced pressure
  5. customThe residue was chromatographed on a silica gel column (LiChroprepDIOL (Merck))

출처 및 근거

ORD 기록
ord-09c6ccdd961e4b6d9517a89f30f242e2
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06596751B2

반응 노트

불러오는 중…